CN107570128A - A kind of industrial waste Al2O3Bead regenerative system and renovation process - Google Patents
A kind of industrial waste Al2O3Bead regenerative system and renovation process Download PDFInfo
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- CN107570128A CN107570128A CN201610526029.2A CN201610526029A CN107570128A CN 107570128 A CN107570128 A CN 107570128A CN 201610526029 A CN201610526029 A CN 201610526029A CN 107570128 A CN107570128 A CN 107570128A
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Abstract
The invention provides a kind of industrial waste Al2O3Bead regenerative system and renovation process, the system include micropore activation system, segmentation regenerative system, waste gas cleaning system and online monitoring system；Wherein, micropore activation system is connected with segmentation regenerative system, and waste gas cleaning system is connected with micropore activation system, and online monitoring system is connected with micropore activation system and segmentation regenerative system.The present invention hydrolyzes solution of silane to discarding Al by nanometer2O3Bead carries out leaching activation process, the metal ion bag inside bead is connect into separation, while the material such as Anthraquinones activation bag in 2 EAQs and DMF is connect；Again by the Al Jing Guo activation process2O3Bead carries out calcine by steps regeneration, and the regeneration Al with superperformance is made2O3Bead, and there is good regeneration rate.
Description
Technical field
The invention belongs to resource recycling field, is related to a kind of industrial waste Al2O3Bead regenerative system and again
Generation method.
Background technology
Hydrogen peroxide is also known as hydrogen peroxide, in chemical industry, pharmaceuticals industry, printing and dyeing industry, intermetallic composite coating, spinning
All many-sides such as fabric is drifted, military project fuel and civilian disinfectant all have extensive and irreplaceable purposes.
The Hydrogen Peroxide Production enterprise in China is except only a few is still in addition to using electrolysis and isopropanol method at present, absolutely mostly
Number is all using (also referred to as anthraquinone) production of 2- EAQs method of comparative maturity.
Anthraquinone technique is that 2- EAQs and organic solvent are configured into working solution, 3atm, 55~65 DEG C and
Catalyst participates in lower hydrogenation hydrogenation, then carries out counter flow oxidation in 40~44 DEG C and air, through extracting, regenerating, essence
Make and be concentrated to give aqueous hydrogen peroxide solution product.It is in last handling process, it is necessary to small using activated alumina
Ball carries out absorption to working solution except alkali and regeneration degradation product, so as to the working solution that can be recycled, and lives
The adsorption process of property alumina globule is then not effectively reversible regeneration.When alumina globule adsorbent uses one section
Between after must change, with ensure working solution regeneration needs.
Used alumina globule adsorbent contains the works such as 2- EAQs, trioctyl phosphate and pseudocumene
Make liquid composition, while be also possible to the Partial digestion product containing working solution component, its color is that quinones substance is normal
That sees is pink → red, shows its dangerous waste content nearly 1/5th, and complicated component according to proportion, regenerated
Journey need to be isolated processing.These discarded alumina globules are burnt as harmful solid waste burning high temperature at present
Burn, the alumina powder after burning is frequently used to make ceramic material, and this makes still to preserve in material more
Pore structure is sintered and lost, and atmosphere pollution is serious.Some Enterprises is reduce cost, directly by aluminum oxide
Bead is stolen and buried, and more causes severe persistent to pollute.
CN 101376100A disclose a kind of activated alumina regeneration of hydrogen peroxide working liquid regenerative process
Processing method, it is specifically：By the failure aluminum oxide drawn off in working solution Regenerative beds in hydrogen peroxide manufacture with
The inert aluminum oxide that burns enters tower reactor from top together, is moved down by gravity, oxygen-containing gas
Enter reactor from the bottom of tower reactor, upwards motion, reacted regenerative aluminium oxide and burning inertia
Aluminum oxide, discharged from the bottom discharge device of reactor, tail gas of the reacted tail gas from reactor top
Floss hole discharges reactor；Reaction temperature is 360~800 DEG C, and the residence time of solid material in the reactor is
3~15 hours.Although the above method is avoided in conventional regeneration technique caused by 1000 DEG C of high temperature above conditions
Al2O3The problem of bead hydraulic performance decline, but it can not effectively remove Al2O3Metal ion in bead with
And anthraquinones, and regeneration efficiency is low.
Therefore, regeneration efficiency height how is found, and the high suitable renovation process of impurity removal efficacy is to this
Class discarded object realizes the key of high added value recycling.
The content of the invention
For problems of the prior art, the invention provides a kind of industrial waste Al2O3Bead regeneration system
System and renovation process, methods described hydrolyze solution of silane to discarding Al by nanometer2O3Bead is leached at activation
Reason, metal ion (such as potassium, sodium, the aluminium and magnesium) bag inside bead is connect into separation, while by 2- ethyls
The activation bag such as anthraquinones connects in anthraquinone and DMF；Again by the Al Jing Guo activation process2O3Bead is divided
Section calcining regenerates, and the regeneration Al with superperformance is made2O3Bead, and there is good regeneration rate.
To use following technical scheme up to this purpose, the present invention：
In a first aspect, the invention provides a kind of industrial waste Al2O3Bead regenerative system, the system include
Micropore activation system, segmentation regenerative system, waste gas cleaning system and regeneration monitoring system；Wherein, micropore is lived
Change system is connected with segmentation regenerative system, and waste gas cleaning system is connected with micropore activation system, regeneration monitoring system
System is connected with micropore activation system and segmentation regenerative system.
In the present invention, the regeneration monitoring system is used to monitor in micropore activation system and segmentation regenerative system
Process conditions, and then each technological parameter is adjusted in real time, obtain a stable activating and regenerating environment.
In the present invention, the industrial waste Al2O3Be adsorbed with bead 2- EAQs, trioctyl phosphate and
The working solutions such as pseudocumene and Partial digestion product, its a diameter of 3~5mm, heap density are 0.95~1.15g/cm3。
It is used as currently preferred technical scheme below, but not as the limitation of technical scheme provided by the invention,
By the following technical programs, it can preferably reach and realize the technical purpose and beneficial effect of the present invention.
As currently preferred technical scheme, the micropore activation system includes pretreatment system, dipping is lived
Change system, circulation liquid mixing system and Transmission system, wherein pretreatment system, impregnating active system and circulation are matched somebody with somebody
Liquid system is sequentially connected, and Transmission system is connected to pretreatment system, impregnating active system and circulation liquid mixing system；
That is, Transmission system is used to transmit discarded Al2O3Bead, make it successively by pretreatment system, impregnating active system
System and circulation liquid mixing system are handled.
Preferably, the pretreatment system includes soot blowing dust collect plant and preheating device.Wherein, the pre- place
Reason system is successively to discarding Al2O3Bead carries out soot blowing and the pre-heat treatment.
Preferably, the impregnating active system includes activating tank.
Preferably, the impregnating active system includes being used for the lowering or hoisting gear that is freely lifted activating tank and heat-insulated
Device, the activating tank and lowering or hoisting gear are respectively positioned in heat-proof device.
Preferably, the impregnating active system includes vacuum extractor, the vacuum extractor and activating tank phase
Even.In the present invention, the priming reaction need to be carried out under condition of negative pressure, thus need to set vacuum extractor.
In the present invention, the activating tank carries the function of water bath with thermostatic control, and activation can be made to carry out at a constant temperature；
The impregnating active system also includes heat-proof device, and the effect of the heat-proof device is activation system is in one
Under individual heat-insulated environment, activation is kept to carry out at a certain temperature.
Preferably, the activating solution in the activating tank is that nanometer hydrolyzes solution of silane.
Preferably, the nanometer hydrolysis solution of silane includes aqueous silane coupling agent, non-ionic surface active
Agent and pH adjusting agent.Wherein, the solvent of nanometer hydrolysis solution of silane is water.
Preferably, the concentration of water-based silane coupler is 1~20wt% in nanometer hydrolysis solution of silane, example
Such as 1wt%, 3wt%, 5wt%, 7wt%, 10wt%, 13wt%, 15wt%, 17wt% or 20wt%,
It is not limited to cited numerical value, other interior numerical value of listed scope are feasible, more preferably
2~10wt%.
Preferably, the concentration of the nonionic surfactant is 0.1~1wt%, such as 0.1wt%, 0.2wt%,
0.3wt%, 0.4wt%, 0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt% or 1wt% etc., but
It is not limited in cited numerical value, other numerical value are feasible in listed scope, more preferably
0.1~0.6wt%.
Preferably, the pH adjusting agent is organic acid, such as acetic acid etc..In the present invention, the organic acid master
Will be as the catalyst of silane hydrolyzate.
Preferably, the dosage of the pH adjusting agent to make pH value of solution be 3~6.5, such as 3,3.5,4,4.5,
5th, 5.5,6 or 6.5 etc., it is not limited to cited numerical value, other interior numerical value of listed scope are feasible.
In the present invention, the activation process need to be controlled in the range of certain pH, i.e., nanometer hydrolyzes solution of silane
PH value need to be maintained at 3~6.5.It is neutral most slow because silane hydrolyzate speed is relevant with pH value in the present invention, partially
Acid or meta-alkali are all very fast, therefore need to typically adjust the pH value of solution, and then adjust hydrolysis rate.In the present invention,
In addition to amino silane, other silane can add a small amount of organic acid, and regulation pH value to 4~5, amino silane is because of tool
Alkalescence, it is not necessary to adjust.
Preferably, the Transmission system includes transmission chain, and it connects pretreatment system, impregnating active system
With circulation liquid mixing system.
Preferably, the circulation liquid mixing system includes precipitation filter, liquid dispensing device and the storage being sequentially connected
Liquid device.The filtering-depositing device is used to the liquid used during impregnating active being collected filtering,
Liquid dispensing device, which is used to filtering the obtained liquid of precipitation, to carry out obtaining nanometer with liquid hydrolyzing solution of silane and is circulated
Utilize, the system for making system of the present invention form zero discharging of waste liquid.
In the present invention, solution of silane is hydrolyzed to Al with nanometer2O3The principle that bead carries out activation process is as follows：
Silane is a kind of hybrid thing containing silicon substrate, and its basic molecular formula is：R'(CH2)nSi(OR)3。
Wherein OR is hydrolyzable group, and R' is organo-functional group.Silane is in aqueous generally in the form of hydrolysis
In the presence of：
-Si(OR)3+H2O=Si (OH)3+3ROH
Pass through its SiOH group and the MeOH groups of metal surface after silane hydrolyzate (Me represents metal)
Shrink reaction and quick adsorption in metal surface, SiOH+MeOH=SiOMe+H2O.On the one hand, silane exists
Si-O-Me covalent bonds are formed on metal interface, in general, active force between covalent bond up to 700kJ/t,
Combination between silane and metal is very firm.Silane hydrolyzes silicon into nano shape, i.e. nanometer after hydrolysis
Alkane, micropore is permeable to by special activation device and forms stable covalent bond with metal, in certain temperature
Excite it is lower metal ion is taken out of, so as to reach the purpose of separation.
Bag connection technology of the present invention refers in the molecule mixture of required processing that moieties performance can not
Meet whole mixt processing requirement, i.e., the heat endurance of molecule and parent, fusing point, chemical reactivity and
Under the conditions of the physical and chemical performances such as dissolubility are distinguishing, connect to form oikocryst compound using unimolecule or polymolecular bag,
Meet the technology for exciting lower molecule and precursor structure to assemble specific compound in specified conditions.
Anthraquinones in alumina globule need more than 1000 DEG C of temperature to be discharged from micropore, but
Under this hot conditions, there is substantial amounts of powder phenomenon-tion in the surface of bead, and performance drastically declines.It is low to realize
Warm regeneration function, the application it has been investigated that, remaining silane molecule is anti-by the polycondensation between SiOH groups
Should metal surface formed with Si-O-Si tridimensional networks silane film, and by side chain reaction technology with
Mowital functional raw materials (Mowital is a kind of free flowable white powder of fine particle shape) are by height
The grafting of hydroformylation molecule connects the activation bag such as anthraquinones of indissoluble into anthraquinone molecular chain, and follow-up
The lower low temperature of microwave triggering of high IR all band pharoid is separated out so that regenerative process is possibly realized.
Micropore activation system activation utilization high efficiency water silane bag connection technology and side chain of the present invention react skill
Art, the ionic gel in alumina globule micropore is fast at high speed into macromolecule, efficiency.
As currently preferred technical scheme, the segmentation regenerative system includes regenerating unit and waste gas purification
Module.
Preferably, the regenerating unit is divided into four sections, is followed successively by low temperature drying area, medium temperature lasing region, high temperature
Renewing zone and normal temperature cooling zone.
Preferably, the regenerating unit includes conveyer, and the conveyer is through the whole regeneration dress of connection
Put, that is, be used to come and go material in low temperature drying area, medium temperature lasing region, high temperature regeneration area and normal temperature cooling zone
Transport.
Preferably, the waste gas purification module includes the low temperature drying area waste gas purification being connected with low temperature drying area
Module, the medium temperature lasing region waste gas purification module being connected with medium temperature lasing region, and be connected with high temperature regeneration area
High temperature regeneration area waste gas purification module.
Preferably, the regenerating unit uses all band electric heating system, is made with all band infrared heating electrical device
For heating element heater.
In the present invention, heating element heater selects high energy full-wave band infrared radiation heater, compared to traditional heating
Energy-saving Tunnel Kiln 30~50%, and the reproduction quality of parent can be ensured.Herein, all band electrical heating system
System and all band infrared heating electrical device are existing device in the prior art, therefore are repeated no more.
Preferably, the operation temperature in the low temperature drying area be 80~110 DEG C, such as 80 DEG C, 83 DEG C, 85 DEG C,
87 DEG C, 90 DEG C, 93 DEG C, 95 DEG C, 97 DEG C, 100 DEG C, 103 DEG C, 105 DEG C, 107 DEG C or 110 DEG C etc., but
It is not limited in cited numerical value, other numerical value are feasible in listed scope, more preferably
90~100 DEG C.
Preferably, the operation temperature of the medium temperature lasing region be 300~600 DEG C, such as 300 DEG C, 330 DEG C,
350℃、370℃、400℃、430℃、450℃、470℃、500℃、530℃、550℃、570℃
Or 600 DEG C etc., it is not limited to cited numerical value, other interior numerical value of listed scope are feasible, further
Preferably 400~500 DEG C.
Preferably, the operation temperature in the high temperature regeneration area be 600~900 DEG C, such as 600 DEG C, 630 DEG C,
650℃、670℃、700℃、730℃、750℃、770℃、800℃、830℃、850℃、870℃
Or 900 DEG C etc., it is not limited to cited numerical value, other interior numerical value of listed scope are feasible, further
Preferably 700~800 DEG C.
Preferably, the operation temperature of the normal temperature cooling zone be 20~30 DEG C, such as 20 DEG C, 21 DEG C, 22 DEG C,
23 DEG C, 25 DEG C, 26 DEG C, 27 DEG C, 28 DEG C, 29 DEG C or 30 DEG C etc., it is not limited to cited numerical value,
Other numerical value are feasible in listed scope.
Preferably, catalytic temperature is used in the low temperature drying area waste gas purification module as 80~110 DEG C of non-gold
Belong to base catalyst.
Preferably, catalytic temperature is used in the medium temperature lasing region waste gas purification module as 300~600 DEG C of non-gold
Belong to base catalyst.
Preferably, catalytic temperature is used in the high temperature regeneration area waste gas purification module as 600~900 DEG C of non-gold
Belong to base catalyst.
Preferably, it is described to return to regenerating unit through waste gas purification module purified gas.
Preferably, the low temperature drying area waste gas purification module purified gas returns to low temperature drying area, institute
State medium temperature lasing region waste gas purification module purified gas and return to medium temperature lasing region, the high temperature regeneration area gives up
Gas cleaning module purified gas returns to high temperature regeneration area.
, can be by by the way of the regenerating unit in the segmentation regenerative system is regenerated using sectional in the present invention
Walk Al2O3Adsorption impurity gradient parsing removing, prevent intersect sintering curing, blocking bridging micropore,
Influence regeneration effect；Secondly, if not being segmented high temperature regeneration, it will a large amount of Thermal desorption organic volatiles are produced,
Concentration is gathered too high, is unfavorable for vent gas treatment, and bring explosion danger.
In the present invention, by waste gas purification module subregion, different subregions are using the catalysis for being applicable different catalytic temperatures
Agent, can make it is purified after gas be maintained within the scope of corresponding temperature, return again to respective correspondence after purification
Regeneration zone, make in the state of the regenerative environ-ment of regeneration zone maintains a temperature, to ensure that revival
Rate.
As currently preferred technical scheme, the waste gas cleaning system includes the washing and filtering being sequentially connected
System, catalytic degradation device and gas extraction system.
Preferably, the catalyst in the catalytic degradation device is multi-layer honeycomb shape catalyst.
Preferably, the multi-layer honeycomb shape catalyst is non-metal base catalyst.
Second aspect, the invention provides above-mentioned industrial waste Al2O3The renovation process of bead regenerative system, institute
The method of stating comprises the following steps：
(1) to discarding Al2O3Bead is activated and dried under condition of negative pressure, and to being produced in activation process
Raw waste liquid is reclaimed and recycled；
(2) to activated dried discarded Al2O3Bead carries out calcination and regeneration processing, obtains regenerating Al2O3
Bead；
(3) purified treatment is carried out to caused waste gas in activation drying and calcination regeneration process.
As currently preferred technical scheme, step (1) is to discarding Al2O3It is right before bead is activated
Discarded Al2O3Bead is pre-processed.
Preferably, the pretreatment includes soot blowing dedusting and preheating.Wherein, the purpose of preheating is prevented in ring
Under the relatively low environment of border process temperature, bead breaks out when outdoor enters device again and ruptured, if outdoor temperature meets
It is required that also can be without preheating.
As currently preferred technical scheme, step (1) is to discarding Al2O3The method that bead is activated
For：By discarded Al2O3Bead is sent into activating tank to be activated with nanometer hydrolysis solution of silane.
Preferably, the nanometer hydrolysis solution of silane includes aqueous silane coupling agent, non-ionic surface active
Agent and pH adjusting agent.
Preferably, the concentration of water-based silane coupler is 1~20wt% in nanometer hydrolysis solution of silane, example
Such as 1wt%, 3wt%, 5wt%, 7wt%, 10wt%, 13wt%, 15wt%, 17wt% or 20wt%,
It is not limited to cited numerical value, other interior numerical value of listed scope are feasible, more preferably
2~10wt%.
Preferably, the concentration of the nonionic surfactant is 0.1~1wt%, such as 0.1wt%, 0.2wt%,
0.3wt%, 0.4wt%, 0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt% or 1wt% etc., but
It is not limited in cited numerical value, other numerical value are feasible in listed scope, more preferably
0.1~0.6wt%.
Preferably, the pH adjusting agent is organic acid, such as acetic acid etc..
Preferably, the dosage of the pH adjusting agent to make pH value of solution be 3~6.5, such as 3,3.5,4,4.5,
5th, 5.5,6 or 6.5 etc., it is not limited to cited numerical value, other interior numerical value of listed scope are feasible.
Preferably, activation pressure is -0.1~0MPa and does not include 0MPa in the activation process, such as
-0.1MPa、-0.09MPa、-0.08MPa、-0.07MPa、-0.06MPa、-0.05MPa、-0.04MPa、
- 0.03MPa, -0.02MPa or -0.01MPa etc., it is not limited to cited numerical value, in listed scope
Other numerical value are feasible, more preferably -0.09~-0.05MPa.In the present invention, the activation is in negative pressure bar
Carried out under part.Activation process of the present invention need to be carried out under condition of negative pressure, if not using condition of negative pressure, meeting
Substantially reduce activating solution depth and penetrate into Al2O3Bead, influence bag and connect, activate and other effects.
Preferably, the soak time≤30s, such as 30s, 25s, 20s, 15s, 10s or 5s etc., but simultaneously
Cited numerical value is not limited only to, other numerical value are feasible in listed scope, more preferably 10~20s.
Preferably, the activation temperature be 50~70 DEG C, such as 50 DEG C, 53 DEG C, 55 DEG C, 57 DEG C, 60 DEG C,
63 DEG C, 65 DEG C, 67 DEG C or 70 DEG C etc., it is not limited to cited numerical value, other interior numbers of listed scope
Value is feasible.
As currently preferred technical scheme, the drying temperature of step (1) described drying is 60~90 DEG C,
Such as 60 DEG C, 63 DEG C, 65 DEG C, 67 DEG C, 70 DEG C, 73 DEG C, 75 DEG C, 77 DEG C, 80 DEG C, 83 DEG C, 85 DEG C,
87 DEG C or 90 DEG C etc., it is not limited to cited numerical value, other interior numerical value of listed scope are feasible, enter
One step is preferably 60~80 DEG C.
Preferably, the drying time of step (1) described drying is 30~50min, such as 30min, 35min,
40min, 45min or 50min etc., more preferably 30~40min.
Preferably, step (1) is described is reclaimed and is recycled to caused waste liquid in activation process, is
By waste liquid successively by precipitation filtering and with liquid after, return activating tank recycled.
Preferably, it is described to be adjusted with liquid to add aqueous silane coupling agent and pH into the solution after precipitation filters
Agent is saved, obtains nanometer hydrolysis solution of silane.
As currently preferred technical scheme, the processing of calcination and regeneration described in step (2) includes low temperature successively
Drying, medium temperature excite, the cooling of high temperature regeneration and normal temperature.
Preferably, the temperature of the low temperature drying be 80~110 DEG C, such as 80 DEG C, 83 DEG C, 85 DEG C, 87 DEG C,
90 DEG C, 93 DEG C, 95 DEG C, 97 DEG C, 100 DEG C, 103 DEG C, 105 DEG C, 107 DEG C or 110 DEG C etc., but simultaneously not only
It is limited to cited numerical value, other numerical value are feasible in listed scope, more preferably 90~110 DEG C.
Preferably, the time of the low temperature drying is 10~60min, for example, 10min, 20min, 30min,
40min, 50min or 60min etc., it is not limited to cited numerical value, other interior numerical value of listed scope
It is feasible, more preferably 20~40min.
Preferably, the temperature that the medium temperature excites be 300~600 DEG C, such as 300 DEG C, 330 DEG C, 350 DEG C,
370 DEG C, 400 DEG C, 430 DEG C, 450 DEG C, 470 DEG C, 500 DEG C, 530 DEG C, 550 DEG C, 570 DEG C or 600 DEG C
Deng it is not limited to cited numerical value, other interior numerical value of listed scope are feasible, more preferably
400~500 DEG C.
Preferably, the time that the medium temperature excites is 20~90min, for example, 20min, 30min, 40min,
50min, 60min, 70min, 80min or 90min etc., it is not limited to cited numerical value, listed
In the range of other numerical value it is feasible, more preferably 30~60min.
Preferably, the temperature of the high temperature regeneration be 600~900 DEG C, such as 600 DEG C, 630 DEG C, 650 DEG C,
670 DEG C, 700 DEG C, 730 DEG C, 750 DEG C, 770 DEG C, 800 DEG C, 830 DEG C, 850 DEG C, 870 DEG C or 900 DEG C
Deng it is not limited to cited numerical value, other interior numerical value of listed scope are feasible, more preferably
700~800 DEG C.
Preferably, the time of the high temperature regeneration is 30~120min, for example, 30min, 40min, 50min,
60min, 70min, 80min, 90min, 100min, 110min or 120min etc., it is not limited to
Cited numerical value, other interior numerical value of listed scope are feasible, more preferably 50~80min.
Preferably, the temperature of normal temperature cooling is 20~30 DEG C, for example, 20 DEG C, 21 DEG C, 22 DEG C, 23 DEG C,
25 DEG C, 26 DEG C, 27 DEG C, 28 DEG C, 29 DEG C or 30 DEG C etc., it is not limited to cited numerical value, listed
In the range of other numerical value it is feasible.
Preferably, the time of normal temperature cooling be 40~160min, such as 40min, 50min, 60min,
70min、80min、90min、100min、110min、120min、130min、140min、150min
Or 160min etc., it is not limited to cited numerical value, other interior numerical value of listed scope are feasible, enter one
Step is preferably 50~80min.
Waste gas caused by being dried as currently preferred technical scheme, in step (3) to activation is sent into waste gas
Cleaning system is purified, and the purification includes handling waste gas washing and filtering and catalytic degradation.
Preferably, the temperature of catalytic degradation processing is 200~500 DEG C, for example, 200 DEG C, 250 DEG C, 300 DEG C,
350 DEG C, 400 DEG C, 450 DEG C or 500 DEG C etc., it is not limited to cited numerical value, in listed scope its
His numerical value is feasible.
Preferably, caused waste gas is sent into segmentation regeneration system in step (3) processing procedure to calcination and regeneration
Waste gas purification module in system carries out segmentation purified treatment.
As currently preferred technical scheme, to activating drying and calcination regeneration treatment in the renovation process
Carry out on-line monitoring.
Preferably, step (2) obtains regenerating Al2O3The heap density of bead is 0.75~0.85g/cm3, compare surface
Product is 200~300m2/g。
More specifically, the renovation process comprises the following steps：
(1) Al is discarded2O3Bead enters micropore activation system, delivers in pretreatment system through Transmission system
The dedusting of row soot blowing and the pre-heat treatment, bead after pretreatment are sent into impregnating active system by Transmission system and existed
Activated and dried under condition of negative pressure, caused waste liquid is sent into circulation liquid mixing system and returned in activation process
Receive and recycle；
(2) activated dried discarded Al2O3The regenerating unit that bead enters in segmentation regenerative system, according to
It is secondary excited through low temperature drying, medium temperature, high temperature regeneration and normal temperature cooling treatment, obtain regenerating Al2O3Bead；
(3) activate caused waste gas in drying process and be sent into waste gas cleaning system progress purified treatment, it is described net
Changing includes handling waste gas washing and filtering and catalytic degradation；It is segmented caused waste gas in regenerative system and is sent into segmentation
Waste gas purification module in regenerative system carries out purified treatment.
Compared with prior art, the invention has the advantages that：
The present invention hydrolyzes solution of silane to discarding Al by nanometer2O3Bead leaches activation process, inside bead
Metal ion (such as potassium, sodium, aluminium and magnesium) bag connect separation, while by anthracene in 2- EAQs and DMF
The materials such as quinones activation bag connects；Again by the Al Jing Guo activation process2O3Bead carries out calcine by steps regeneration, is made
Regeneration Al with superperformance2O3Bead, gained Al2O3The heap density of bead is 0.75~0.85g/cm3,
Specific surface area is 200~300m2/ g, the content of its remaining metal ion are less than 10 μ g/g, remaining carbon content
Less than 3 μ g/g, and there is good regeneration rate, regeneration efficiency is up to more than 99%.
Brief description of the drawings
Fig. 1 is industrial waste Al described in embodiment 12O3The structure of micropore activation system is shown in bead regenerative system
It is intended to；
Fig. 2 is industrial waste Al described in embodiment 12O3The side view knot of micropore activation system in bead regenerative system
Structure schematic diagram；
Fig. 3 is the structural representation that liquid mixing system is circulated in micropore activation system described in embodiment 1；
Fig. 4 is industrial waste Al described in embodiment 12O3The structure for being segmented regenerative system in bead regenerative system is shown
It is intended to；
Fig. 5 is industrial waste Al described in embodiment 12O3The vertical view knot of regenerative system is segmented in bead regenerative system
Structure schematic diagram；
Fig. 6 is industrial waste Al described in embodiment 12O3The side view knot of regenerative system is segmented in bead regenerative system
Structure schematic diagram；
Wherein, 1- soot blowings dust collect plant, 2- preheating devices, 3- activating tanks, 4- lowering or hoisting gears, 5- heat-proof devices,
6- transmission chains, 7- collecting tanks, 8- precipitation filters, 9- liquid dispensing devices, 10- sump assemblies, 11- low temperature
Baking zone, 12- medium temperature lasing regions, 13- high temperature regenerations area, 14- normal temperature cooling zone, 15- conveyers, 16-
Low temperature drying area waste gas purification module, 17- medium temperature lasing region waste gas purification modules, 18- high temperature regenerations area waste gas are net
Change module, 19- heating element heaters.
Embodiment
For the present invention is better described, technical scheme is readily appreciated, it is further to the present invention below
Describe in detail.But following embodiments is only the simple example of the present invention, the present invention is not represented or limited
Rights protection scope, the scope of the present invention is defined by claims.
Embodiment 1：
Present embodiments provide a kind of industrial waste Al2O3Bead regenerative system, the system activate including micropore
System, segmentation regenerative system, waste gas cleaning system and online monitoring system；Wherein, micropore activation system with
Segmentation regenerative system is connected, and waste gas cleaning system is connected with micropore activation system, online monitoring system and micropore
Activation system is connected with segmentation regenerative system.
The micropore activation system includes pretreatment system, impregnating active system, circulation liquid mixing system and transmission
System, wherein pretreatment system, impregnating active system and circulation liquid mixing system are sequentially connected, and Transmission system connects
It is connected to pretreatment system, impregnating active system and circulation liquid mixing system.
As depicted in figs. 1 and 2, the pretreatment system includes soot blowing dust collect plant 1 and preheating device 2；Institute
Stating impregnating active system includes activating tank 3, in addition to for making the He of lowering or hoisting gear 4 that activating tank can be freely lifted
Heat-proof device 5, the activating tank 3 and lowering or hoisting gear 4 are respectively positioned in heat-proof device 5；The impregnating active system
System includes vacuum extractor, and the vacuum extractor is connected with activating tank 3；The Transmission system includes transmission
Chain 6, it connects pretreatment system, impregnating active system and circulation liquid mixing system.
As shown in figure 3, it is described circulation liquid mixing system include be sequentially connected collecting tank 7, precipitation filter 8,
Liquid dispensing device 9 and sump assemblies 10.
The segmentation regenerative system includes regenerating unit and waste gas purification module.
As shown in Figure 4 and Figure 6, the regenerating unit is divided into four sections, is followed successively by low temperature drying area 11, medium temperature
Lasing region 12, high temperature regeneration area 13 and normal temperature cooling zone 14；The regenerating unit also includes conveyer 15,
The conveyer 15 is through the whole regenerating unit of connection；The regenerating unit uses all band electric heating system,
Heating element heater 19 is used as using all band infrared heating electrical device.
As shown in figure 5, the waste gas purification module includes the low temperature drying area waste gas being connected with low temperature drying area
Cleaning module 16, the medium temperature lasing region waste gas purification module 17 being connected with medium temperature lasing region, and with high temperature again
The connected high temperature regeneration area waste gas purification module 18 in raw area.
The waste gas cleaning system includes washing and filtering system, catalytic degradation device and the exhaust system being sequentially connected
System；Catalyst in the catalytic degradation device is multi-layer honeycomb shape catalyst.
Embodiment 2：
The present embodiment is using the industrial waste Al described in embodiment 12O3Bead regenerative system is to industrial waste
Al2O3Bead is regenerated, the discarded Al2O3Bead be adsorbed with 2- EAQs, trioctyl phosphate, partially
The working solutions such as trimethylbenzene and Partial digestion product, 3~5mm of diameter, discard Al2O3The heap density of bead
0.95~1.15g/cm3。
It the described method comprises the following steps：
(1) by discarded Al2O3Bead is sent into micropore activation system, and pretreatment system is delivered to by transmission chain 6
Soot blowing dedusting is carried out through soot blowing dust collect plant 1 and preheated device 2 is preheated in system, it is after pretreatment
Bead by transmission chain 6 be sent into impregnating active system pressure be -0.05MPa under the conditions of in activating tank 3
15s, Al after activation are activated at 60 DEG C2O3At bead drying 35min at 70 DEG C, activation process and drying
Caused waste liquid is sent into circulation liquid mixing system and is reclaimed and recycled in reason；
Wherein, the activating solution in activating tank 3 is that nanometer hydrolyzes solution of silane, including the water that concentration is 10wt%
Property silane coupler, 0.5wt% nonionic surfactant and pH adjusting agent acetic acid, the dosage of acetic acid is makes
PH value of solution is 4.
(2) activated dried discarded Al2O3The regenerating unit that bead enters in segmentation regenerative system, according to
It is secondary to excite 50min, 750 DEG C of high temperature regeneration 60min and 25 DEG C through 100 DEG C of low temperature drying 50min, 500 DEG C of medium temperatures
Normal temperature cooling treatment 70min, obtain regenerate Al2O3Bead；
(3) activate caused waste gas in drying process and be sent into waste gas cleaning system progress purified treatment, it is described net
Changing includes handling waste gas washing and filtering and catalytic degradation；It is segmented caused waste gas in regenerative system and is sent into segmentation
Waste gas purification module in regenerative system carries out purified treatment.
The Al for handling to obtain by the present embodiment methods described2O3The heap density of bead is 0.85g/cm3, compare table
Area is 208m2/ g, regeneration efficiency 99.8%.
Embodiment 3：
The present embodiment is using the industrial waste Al described in embodiment 12O3Bead regenerative system is to industrial waste
Al2O3Bead is regenerated, the industrial waste Al2O3Bead is as described in Example 2.
It the described method comprises the following steps：
(1) by discarded Al2O3Bead is sent into micropore activation system, and pretreatment system is delivered to by transmission chain 6
Soot blowing dedusting is carried out through soot blowing dust collect plant 1 and preheated device 2 is preheated in system, it is after pretreatment
Bead by transmission chain 6 be sent under the conditions of impregnating active system pressure is -0.07MPa in activating tank 3 in
30s, Al after activation are activated at 50 DEG C2O3Bead dries 50min, activation process and drying process at 60 DEG C
In caused waste liquid be sent into circulation liquid mixing system and reclaimed and recycled；
Wherein, the activating solution in activating tank 3 is that nanometer hydrolyzes solution of silane, including the water that concentration is 20wt%
Property silane coupler, 0.6wt% nonionic surfactant and pH adjusting agent acetic acid, the dosage of acetic acid is makes
PH value of solution is 6.5.
(2) activated dried discarded Al2O3The regenerating unit that bead enters in segmentation regenerative system, according to
It is secondary to excite 30min, 900 DEG C of high temperature regeneration 50min and 30 DEG C through 110 DEG C of low temperature drying 20min, 600 DEG C of medium temperatures
Normal temperature cooling treatment 50min, obtain regenerate Al2O3Bead；
(3) activate caused waste gas in drying process and be sent into waste gas cleaning system progress purified treatment, it is described net
Changing includes handling waste gas washing and filtering and catalytic degradation；It is segmented caused waste gas in regenerative system and is sent into segmentation
Waste gas purification module in regenerative system carries out purified treatment.
The Al for handling to obtain by the present embodiment methods described2O3The heap density of bead is 0.75g/cm3, compare table
Area is 293m2/ g, regeneration efficiency 99.4%.
Embodiment 4：
The present embodiment is using the industrial waste Al described in embodiment 12O3Bead regenerative system is to industrial waste
Al2O3Bead is regenerated, the industrial waste Al2O3Bead is as described in Example 2.
It the described method comprises the following steps：
(1) by discarded Al2O3Bead is sent into micropore activation system, and pretreatment system is delivered to by transmission chain 6
Soot blowing dedusting is carried out through soot blowing dust collect plant 1 and preheated device 2 is preheated in system, it is after pretreatment
Bead by transmission chain 6 be sent into impregnating active system pressure be -0.09MPa under the conditions of in activating tank 3
20s, Al after activation are activated at 70 DEG C2O3Bead, which is carried out at 80 DEG C, dries 40min, activation process and dry
Caused waste liquid is sent into circulation liquid mixing system and is reclaimed and recycled in dry processing；
Wherein, the activating solution in activating tank 3 is that nanometer hydrolyzes solution of silane, including concentration is the water-based of 1wt%
Silane coupler, 0.1wt% nonionic surfactant and pH adjusting agent acetic acid, the dosage of acetic acid are molten to make
Liquid pH is 3.
(2) activated dried discarded Al2O3The regenerating unit that bead enters in segmentation regenerative system, according to
It is secondary to excite 60min, 600 DEG C of high temperature regeneration 80min and 20 DEG C through 80 DEG C of low temperature drying 40min, 300 DEG C of medium temperatures
Normal temperature cooling treatment 80min, obtain regenerate Al2O3Bead；
(3) activate caused waste gas in drying process and be sent into waste gas cleaning system progress purified treatment, it is described net
Changing includes handling waste gas washing and filtering and catalytic degradation；It is segmented caused waste gas in regenerative system and is sent into segmentation
Waste gas purification module in regenerative system carries out purified treatment.
The Al for handling to obtain by the present embodiment methods described2O3The heap density of bead is 0.83g/cm3, compare table
Area is 247m2/ g, regeneration efficiency 99.6%.
Embodiment 5：
The present embodiment is using the industrial waste Al described in embodiment 12O3Bead regenerative system is to industrial waste
Al2O3Bead is regenerated, the industrial waste Al2O3Bead is as described in Example 2.
Methods described except in step (1) activation pressure be -0.1MPa, activation temperature is 60 DEG C, during activation
Between be 10s, drying temperature is 90 DEG C, drying time 30min, nonionic surfactant in activating solution
Concentration is that unclassified stores dosage is in the same manner as in Example 2 with method outside 1wt%.
The Al for handling to obtain by the present embodiment methods described2O3The heap density of bead is 0.81g/cm3, compare table
Area is 253m2/ g, regeneration efficiency 99.5%.
Comparative example 1：
This comparative example provides a kind of industrial waste Al2O3Bead renovation process, Al is discarded in methods described2O3
For bead in addition to being activated without micropore, unclassified stores dosage is in the same manner as in Example 2 with renovation process.
The Al for handling to obtain by this comparative example methods described2O3The heap density of bead is 0.91g/cm3, compare table
Area is 156m2/ g, regeneration efficiency 66.3%.
Comparative example 2：
This comparative example provides a kind of industrial waste Al2O3Bead renovation process, Al is discarded in methods described2O3
Bead is not segmented except regeneration treatment, i.e., outer, unclassified stores dosage and again is only calcined at 600~900 DEG C
Generation method is in the same manner as in Example 2.
The Al for handling to obtain by this comparative example methods described2O3The heap density of bead is 0.88g/cm3, compare table
Area is 188m2/ g, regeneration efficiency 87.1%.
It is molten by nanometer hydrolysising silane that integrated embodiment 1-5 and comparative example 1-2 result can be seen that the present invention
Liquid is to discarding Al2O3Bead leaches activation process, by metal ion (such as potassium, sodium, aluminium and the magnesium inside bead
Deng) purification ＆ isolation, while the activation bag such as anthraquinones in 2- EAQs and DMF is connect；It will pass through again
The Al of activation process2O3Bead carries out calcine by steps regeneration, and the regeneration Al with superperformance is made2O3Bead,
Gained Al2O3The heap density of bead is 0.75~0.85g/cm3, specific surface area is 200~300m2/ g, it is remaining
The content of metal ion be less than 10 μ g/g, remaining carbon content is less than 3 μ g/g, and has good regeneration
Rate, regeneration efficiency is up to more than 99%.
Applicant states that the present invention illustrates the method detailed of the present invention, but the present invention by above-described embodiment
Above-mentioned method detailed is not limited to, that is, does not mean that the present invention has to rely on above-mentioned method detailed and could implemented.
Person of ordinary skill in the field is it will be clearly understood that any improvement in the present invention, to each original of product of the present invention
The equivalence replacement of material and the addition of auxiliary element, the selection of concrete mode etc., all fall within the protection model of the present invention
Within the scope of enclosing and disclosing.
Claims (10)
- A kind of 1. industrial waste Al2O3Bead regenerative system, it is characterised in that the system is lived including micropore Change system, segmentation regenerative system, waste gas cleaning system and online monitoring system；Wherein, micropore activation system With segmentation regenerative system be connected, waste gas cleaning system is connected with micropore activation system, online monitoring system with it is micro- Hole activation system is connected with segmentation regenerative system.
- 2. system according to claim 1, it is characterised in that the micropore activation system includes pre- place Reason system, impregnating active system, circulation liquid mixing system and Transmission system, wherein pretreatment system, dipping are lived Change system and circulation liquid mixing system are sequentially connected, and Transmission system is connected to pretreatment system, impregnating active system With circulation liquid mixing system；Preferably, the pretreatment system includes soot blowing dust collect plant (1) and preheating device (2)；Preferably, the impregnating active system includes activating tank (3)；Preferably, the impregnating active system includes being used to make the lowering or hoisting gear (4) that activating tank (3) is freely lifted With heat-proof device (5), the activating tank (3) and lowering or hoisting gear (4) are respectively positioned in heat-proof device (5)；Preferably, the impregnating active system includes vacuum extractor, the vacuum extractor and activating tank (3) It is connected；Preferably, the activating solution in the activating tank (3) is that nanometer hydrolyzes solution of silane；Preferably, the nanometer hydrolysis solution of silane includes aqueous silane coupling agent, non-ionic surface active Agent and pH adjusting agent；Preferably, the concentration of water-based silane coupler is 1~20wt% in the nanometer hydrolysis solution of silane, is entered One step is preferably 2~10wt%；Preferably, the concentration of the nonionic surfactant is 0.1~1wt%, more preferably 0.1~0.6wt%；Preferably, the pH adjusting agent is organic acid；Preferably, the dosage of the pH adjusting agent is to make pH value of solution be 3~6.5；Preferably, the Transmission system includes transmission chain (6), and it connects pretreatment system, impregnating active System and circulation liquid mixing system；Preferably, it is described circulation liquid mixing system include be sequentially connected collecting tank (7), precipitation filter (8), Liquid dispensing device (9) and sump assemblies (10).
- 3. system according to claim 1 or 2, it is characterised in that the segmentation regenerative system includes Regenerating unit and waste gas purification module；Preferably, the regenerating unit is divided into four sections, be followed successively by low temperature drying area (11), medium temperature lasing region (12), High temperature regeneration area (13) and normal temperature cooling zone (14)；Preferably, the regenerating unit includes conveyer (15), and the conveyer (15) is through connection Whole regenerating unit；Preferably, the low temperature drying area that the waste gas purification module includes being connected with low temperature drying area (11) gives up Gas cleaning module (16), the medium temperature lasing region waste gas purification module (17) being connected with medium temperature lasing region (12), And the high temperature regeneration area waste gas purification module (18) being connected with high temperature regeneration area (13)；Preferably, the regenerating unit uses all band electric heating system, is made with all band infrared heating electrical device For heating element heater (19)；Preferably, the operation temperature of the low temperature drying area (11) is 80~110 DEG C, more preferably 90~100 DEG C；Preferably, the operation temperature of the medium temperature lasing region (12) is 300~600 DEG C, more preferably 400~500 DEG C；Preferably, the operation temperature of the high temperature regeneration area (13) is 600~900 DEG C, more preferably 700~800 DEG C；Preferably, the operation temperature of the normal temperature cooling zone (14) is 20~30 DEG C；Preferably, catalytic temperature is used as 80~110 DEG C in the low temperature drying area waste gas purification module (16) Non-metal base catalyst；Preferably, catalytic temperature is used as 300~600 DEG C in the medium temperature lasing region waste gas purification module (17) Non-metal base catalyst；Preferably, catalytic temperature is used as 600~900 DEG C in the high temperature regeneration area waste gas purification module (18) Non-metal base catalyst；Preferably, it is described to return to regenerating unit through waste gas purification module purified gas；Preferably, low temperature drying area waste gas purification module (16) purified gas returns to low temperature drying Area (11), medium temperature lasing region waste gas purification module (17) purified gas return to medium temperature lasing region (12), High temperature regeneration area waste gas purification module (18) purified gas returns to high temperature regeneration area (13).
- 4. according to the system described in claim any one of 1-3, it is characterised in that the waste gas cleaning system Including washing and filtering system, catalytic degradation device and the gas extraction system being sequentially connected；Preferably, the catalyst in the catalytic degradation device is multi-layer honeycomb shape catalyst；Preferably, the multi-layer honeycomb shape catalyst is non-metal base catalyst.
- 5. according to the renovation process of any one of the claim 1-4 systems, it is characterised in that methods described Comprise the following steps：(1) to discarding Al2O3Bead is activated and dried under condition of negative pressure, and to being produced in activation process Raw waste liquid is reclaimed and recycled；(2) to activated dried discarded Al2O3Bead carries out calcination and regeneration processing, obtains regenerating Al2O3 Bead；(3) purified treatment is carried out to caused waste gas in activation drying and calcination regeneration process.
- 6. renovation process according to claim 5, it is characterised in that step (1) is to discarding Al2O3 Before bead is activated, to discarding Al2O3Bead is pre-processed；Preferably, the pretreatment includes soot blowing dedusting and preheating.
- 7. the renovation process according to claim 5 or 6, it is characterised in that step (1) is to discarded Al2O3The method that bead is activated is：By discarded Al2O3Bead is sent into activating tank and uses nanometer hydrolysising silane Solution is activated；Preferably, the nanometer hydrolysis solution of silane includes aqueous silane coupling agent, non-ionic surface active Agent and pH adjusting agent；Preferably, the concentration of water-based silane coupler is 1~20wt% in the nanometer hydrolysis solution of silane, is entered One step is preferably 2~10wt%；Preferably, the concentration of the nonionic surfactant is 0.1~1wt%, more preferably 0.1~0.6wt%；Preferably, the pH adjusting agent is organic acid；Preferably, the dosage of the pH adjusting agent is to make pH value of solution be 3~6.5；Preferably, activation pressure is -0.1~0MPa and does not include 0MPa in the activation process, further excellent Elect -0.09~-0.05MPa as；Preferably, the soak time≤30s, more preferably 10~20s；Preferably, the activation temperature is 50~70 DEG C.
- 8. according to the renovation process described in claim any one of 5-7, it is characterised in that step (1) institute Dry drying temperature is stated as 60~90 DEG C, more preferably 60~80 DEG C；Preferably, the drying time of step (1) described drying is 30~50min, more preferably 30~40min；Preferably, step (1) is described is reclaimed and is recycled to caused waste liquid in activation process, is By waste liquid successively by precipitation filtering and with liquid after, return activating tank recycled；Preferably, it is described even to add aqueous silane into the solution after precipitation and ion-exchange filtration with liquid Join agent and pH adjusting agent, obtain nanometer hydrolysis solution of silane.
- 9. according to the renovation process described in claim any one of 5-8, it is characterised in that in step (2) The calcination and regeneration processing includes low temperature drying successively, medium temperature excites, the cooling of high temperature regeneration and normal temperature；Preferably, the temperature of the low temperature drying is 80~110 DEG C, more preferably 90~110 DEG C；Preferably, the time of the low temperature drying is 10~60min, more preferably 20~40min；Preferably, the temperature that the medium temperature excites is 300~600 DEG C, more preferably 400~500 DEG C；Preferably, the time that the medium temperature excites is 20~90min, more preferably 30~60min；Preferably, the temperature of the high temperature regeneration is 600~900 DEG C, more preferably 700~800 DEG C；Preferably, the time of the high temperature regeneration is 30~120min, more preferably 50~80min；Preferably, the temperature of the normal temperature cooling is 20~30 DEG C；Preferably, the time of the normal temperature cooling is 40~160min, more preferably 50~80min.
- 10. according to the renovation process described in claim any one of 5-9, it is characterised in that in step (3) Waste gas caused by being dried to activation is sent into waste gas cleaning system and purified, and the purification includes washing waste gas Filtering and catalytic degradation processing；Preferably, the temperature of the catalytic degradation processing is 200~500 DEG C；Preferably, caused waste gas is sent into segmentation regeneration system in step (3) processing procedure to calcination and regeneration Waste gas purification module in system carries out segmentation purified treatment；Preferably, on-line monitoring is carried out to activation drying and calcination regeneration treatment in the renovation process；Preferably, step (2) obtains regenerating Al2O3The heap density of bead is 0.75~0.85g/cm3, compare table Area is 200~300m2/g。
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